US7597529B2 - Method for filling a vertical tube with catalyst particles - Google Patents

Method for filling a vertical tube with catalyst particles Download PDF

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Publication number
US7597529B2
US7597529B2 US10/568,613 US56861306A US7597529B2 US 7597529 B2 US7597529 B2 US 7597529B2 US 56861306 A US56861306 A US 56861306A US 7597529 B2 US7597529 B2 US 7597529B2
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United States
Prior art keywords
catalyst particles
filling aid
tube
filling
spacers
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Expired - Fee Related, expires
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US10/568,613
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English (en)
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US20060233631A1 (en
Inventor
Volker Diehl
Steffen Rissel
Silke Berndt
Mark Duda
Knut Eger
Markus Hoelzle
Veron Nsunda
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BASF SE
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BASF SE
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Assigned to BASF AKTIENGESELLSCHAFT reassignment BASF AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BERNDT, SILKE, DIEHL, VOLKER, DUDA, MARK, EGER, KNUT, HOELZLE, MARKUS, RISSEL, STEFFEN, NSUNDA, VERON
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
    • B65G69/00—Auxiliary measures taken, or devices used, in connection with loading or unloading
    • B65G69/16—Preventing pulverisation, deformation, breakage, or other mechanical damage to the goods or materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/003—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor in a downward flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00752—Feeding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00769—Details of feeding or discharging
    • B01J2208/00778—Kinetic energy reducing devices in the flow channel

Definitions

  • the present invention relates to a method of charging a vertical tube with catalyst particles.
  • Such catalyst-filled tubes are employed for carrying out various catalytic gas-phase reactions. Depending on the type of catalyzed reaction, the tubes are heated from the outside or are surrounded by a heat transfer medium such as a salt melt to remove heat.
  • the catalyst particles either consist of a catalytically active composition which has been shaped, with or without use of suitable binders, by extrusion, tableting or the like to give shaped bodies (all-active catalysts) or they comprise a catalytically active composition which is applied in the form of a shell to an inert support (coated catalysts). They can be in the form of spheres, rings, cylinders, cubes, cuboids, or other geometric bodies.
  • catalyst particles When the catalyst particles are introduced into the tube, catalyst particles can break or the catalytic active composition can be partly detached from the support as a result of mechanical stress, depending on the lateral compressive strength and the fracture strength of the catalysts used.
  • the fragments or abraded material formed increase the density of the catalyst bed and during later operation of the tube reactors lead in a disadvantageous fashion to increased pressure drops.
  • EP-A 548 999 describes a method of charging tubes in which the catalyst particles are introduced along a string having flexible bristles which extend in the transverse direction and are located at a distance from one another.
  • the filling aid used here is a flexible body, e.g. a hemp rope, to which oblique blades are affixed.
  • this object is achieved by a method of charging a vertical tube having an internal diameter of 50 mm or less, preferably 40 mm or less, in particular from 20 to 30 mm, with catalyst particles, which comprises
  • the filling aid has no elements such as bristles or blades which extend radially outward from the flexible body and whose projection onto a plane perpendicular to the longitudinal direction of the filling aid has a larger area than the cross section of the flexible body, preferably greater than half the cross section of the flexible body.
  • the filling aid has spacers extending perpendicular to the longitudinal direction of the filling aid, the area of their projection is negligible compared to the cross section of the flexible body.
  • the flexible elongated body of the filling aid can be, for example, a string, a tape or a rope.
  • the flexible body comprises a textile string or a textile tape, e.g. braided natural or synthetic fibers such as nylon.
  • ropes made of metal wires e.g. a stainless steel rope, are likewise suitable.
  • the flexible elongated body has an essentially circular cross section.
  • the ratio of the diameter of the flexible elongated body to the diameter of the tube is preferably from 0.1 to 0.3, more preferably from 0.1 to 0.25.
  • Suitable bodies are, for example, nylon strings having diameters of from about 2.5 to 5 mm, including noncircular cross sections, e.g. Bonder 0.5-2/5-10 mm.
  • filling aids whose flexible elongated body has a noncircular, e.g. rectangular, cross section.
  • tapes having a thickness of from 0.5 to 2 mm and a width of from 5 to 10 mm can be used successfully.
  • the filling aid preferably has a rigid terminating element (element 4 in FIG. 1 and FIG. 2 ) whose density is greater than that of the flexible body at its lower end. Introduction of the filling aid into the tube is aided by such a terminating element.
  • the filling aid can be uniform over the length introduced into the tube.
  • the filling aid is then a smooth filling aid without dampers, spacers or the like.
  • spacers which are located at a distance from one another and extend perpendicular to the longitudinal direction of the filling aid. Such spacers ensure that the filling aid always hangs essential centrally in the tube.
  • the spacers are preferably very thin in order to minimize the risk of blockage caused by descending catalyst particles.
  • the filling aid is withdrawn stepwise or continuously from the tube as the introduction of catalyst particles progresses, so that the lower end of the filling aid is always above the fill height of the catalyst particles in the tube.
  • a suitable procedure comprises:
  • the filling aid is introduced into the tube so that its lower end divides the tube length in any desired ratio, a first layer of catalyst particles is introduced into the tube to below the end of the filling aid, the filling aid is withdrawn from the tube and a second layer of (identical or different) catalyst particles is introduced into the tube. It has been found that when this embodiment of the method is employed, the pressure drop is up to 10% lower than when the tube is charged without the filling aid.
  • the filling aid initially extends into the tube to 2 ⁇ 3 of the length of the tube, catalyst particles are then introduced to below the lower end of the filling aid, the filling aid is then withdrawn to 1 ⁇ 3 of the length of the tube, catalyst particles are then introduced to below the lower end of the filling aid, the filling aid is then fully withdrawn and the tube is then filled completely with catalyst particles. It has been found that this embodiment of the method is advantageous in the case of tube lengths of from three to eight meters. During operation of the tube reactor, the pressure drops were up to 20% lower than when charging methods in which the catalyst particles are introduced without a filling aid were employed.
  • the filling aid initially extends into the tube over essentially the entire length of the tube. Catalyst particles are then introduced and the filling aid is simultaneously withdrawn from the tube at a rate corresponding to the increase in the fill height of the catalyst particles. It has been found that in the case of tube lengths of from three to six meters, this embodiment of the method results in a pressure drop which is up to 40% lower than when the tube is charged without a filling aid.
  • the catalyst particles are preferably introduced into the tube at an essentially constant speed, in particular by means of suitable filling machines.
  • suitable filling machines are generally made for simultaneously charging a plurality of tubes. They have a hopper having a plurality of chambers from which the catalyst particles are injected onto an inclined vibratory chute. When the vibratory chute is started up, the catalyst particles slide uniformly over the chute and drop through holes in the chute into the tubes located underneath.
  • the catalyst particles generally have a (maximum) diameter of from 2 to 15 mm, preferably from 3 to 8 mm.
  • All-active catalysts consist of a catalytically active composition which is shaped, with or without use of suitable binders, by extrusion, tableting or other methods to give shaped bodies such as extrudates, pellets or the like.
  • Coated catalysts comprise a catalytic composition, generally a mixed metal oxide, applied in the form of a shell to an inert support. They can be in the form of spheres, rings, cylinders, cubes, cuboids or other geometric bodies.
  • Such catalysts are known per se and are employed, for example, for the preparation of unsaturated aliphatic carboxylic acids or aldehydes, e.g. acrylic acid, methacrylic acid or acrolein, by gas-phase oxidation of aldehydes, alkanes or alkenes; the preparation of nitrites such as acrylonitrile, methacrylonitrile by ammoxidation of alkanes or alkenes or the preparation of aromatic carboxylic acids or anhydrides, e.g. benzoic acid or phthalic anhydride, by gas-phase oxidation of aromatic hydrocarbons such as toluene, o-xylene or naphthalene.
  • Further catalysts are catalysts which catalyze hydrogenations of a variety of types or catalysts for the synthesis of methanol from synthesis gas.
  • FIG. 1 shows a section through a tube into which a filling aid according to a first embodiment has been hung.
  • FIG. 2 is a schematic showing of a section through a tube into which a filling aid according to a second embodiment has been hung.
  • FIG. 3 shows a section through a tube into which a filling aid that does not have a rigid terminating element according to a third embodiment has been hung.
  • FIG. 4 shows a section through a tube into which a filling aid that does not have a rigid terminating element according to a third embodiment has been hung.
  • a tube 1 is charged with catalyst particles 2 .
  • a plurality of parallel tubes 1 form a shell-and-tube reactor which is suitable for carrying out gas-phase oxidation reactions.
  • a flexible string 3 which serves as filling aid is introduced into the tube.
  • the string shown in FIG. 1 and FIG. 3 is a smooth string without spacers, while the string shown in FIG. 2 and FIG. 4 is a string into which spacers 5 have been introduced at regular intervals.
  • catalyst particles 2 are poured into the tube 1 .
  • transport device 6 for the catalyst particles 2 it is possible to use either a vibratory chute or a conveyor belt.
  • any number of tubes can be charged simultaneously by combining a plurality of transport devices operating in parallel. In this case, it is possible to use automatic unrolling devices which introduce the strings 3 into the tubes 1 and withdraw them again.
  • the tubes are charged by means of charging machines which introduce the catalyst particles into the tubes by means of vibration from a stock vessel via a vibratory chute.
  • a tube having an internal diameter of 25 mm and a length of 4500 mm is charged with 2160 g of a catalyst (ring shape; external diameter ⁇ height ⁇ internal diameter: 7 ⁇ 7 ⁇ 4 mm) without a filling aid. Charging took about 1 minute. The differential pressure established when 2000 standard l/h of air (20° C.) were passed through was then determined.
  • Example 1 was repeated, but a nylon string having a diameter of 4 mm and weighted at the end was allowed to hang into the tube to a depth of 2600 mm, 720 g of catalyst were introduced, the string was withdrawn so that it hung into the tube to a depth of 1200 mm, a further 720 g of catalyst were introduced, the string was removed and a further 720 g of catalyst were introduced. Charging took about 20 s for each of the layers introduced.
  • Example 1 was repeated, but a nylon string having a diameter of 4 mm and weighted at the end was allowed to hang into the tube to a depth of 2000 mm, 1080 g of catalyst were introduced, the string was removed and a further 1080 g of catalyst were introduced. Charging took about 30 s for each of the layers introduced.
  • Example 1 was repeated, but a nylon string having a diameter of 4 mm and weighted at the end was allowed to hang into the tube to a depth of 4300 mm. 2160 g of catalyst were introduced and the string was pulled continuously from the tube as charging progressed. Charging took about 1 minute.
  • a catalyst (ring shape; external diameter ⁇ height ⁇ internal diameter: 5.5 ⁇ 3 ⁇ 3 mm) were allowed to drop into a tube having an internal diameter of 21 mm and a length of 6400 mm and the proportion of fractured catalyst particles was determined.
  • a tube having an internal diameter of 21 mm and a length of 6400 mm was charged with a catalyst (ring shape; external diameter ⁇ height ⁇ internal diameter; 5.5 ⁇ 3 ⁇ 3 mm) to a fill height of 6000 mm. Charging took about 4 minutes.
  • Example 6 was repeated, but a nylon string having a diameter of 4 mm and weighted at the end was allowed to hang into the tube to a depth of 3500 mm, 630 g of catalyst were introduced, the string was removed and a further 620 g of catalyst were introduced and the amount of catalyst was then brought to a fill height of 6000 mm. Charging took about 2 minutes for each of the layers introduced.
  • Comparison of example 6 and example 7 shows that the catalyst bed in example 7 is looser (lower bulk density) and leads to a smaller differential pressure.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Catalysts (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US10/568,613 2003-08-19 2004-08-17 Method for filling a vertical tube with catalyst particles Expired - Fee Related US7597529B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10337998A DE10337998A1 (de) 2003-08-19 2003-08-19 Verfahren zum Befüllen eines vertikalen Rohres mit Katalysatorteilchen
DE103379983 2003-08-19
PCT/EP2004/009226 WO2005018791A1 (de) 2003-08-19 2004-08-17 Verfahren zum befüllen eines vertikalen rohres mit katalysatorteilchen

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Publication Number Publication Date
US20060233631A1 US20060233631A1 (en) 2006-10-19
US7597529B2 true US7597529B2 (en) 2009-10-06

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Country Status (9)

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US (1) US7597529B2 (de)
EP (1) EP1675675A1 (de)
CN (1) CN100522334C (de)
AR (1) AR045276A1 (de)
CA (1) CA2535357A1 (de)
DE (1) DE10337998A1 (de)
TW (1) TWI336681B (de)
WO (1) WO2005018791A1 (de)
ZA (1) ZA200602209B (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080298932A1 (en) * 2007-06-01 2008-12-04 Paul Fry Catalyst Loading System
US20090097958A1 (en) * 2007-10-15 2009-04-16 Tubemaster, Inc. Device and method for transporting catalyst to a reactor vessel
US20100175775A1 (en) * 2007-08-13 2010-07-15 Unidense Technology Gmbh Catalyst loading system
US20100218843A1 (en) * 2007-08-13 2010-09-02 Unidense Technology Gmbh process and device for filling a tube with granular material
RU2809250C2 (ru) * 2019-03-29 2023-12-08 Мицубиси Кемикал Корпорейшн Способ загрузки гранул

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005010645A1 (de) 2005-03-08 2005-08-04 Basf Ag Verfahren zum Befüllen eines Reaktors
GB0520088D0 (en) * 2005-10-04 2005-11-09 Johnson Matthey Plc Catalyst loading apparatus
US7712490B2 (en) * 2006-03-16 2010-05-11 Clean Harbors Catalyst Technologies, Llc Method and apparatus for loading catalyst
WO2009076374A1 (en) * 2007-12-11 2009-06-18 Tubemaster Inc Device and process for precision loading of particles in a vertical tube chemical reactor
EP2306812A4 (de) * 2008-07-30 2013-02-20 Univ Kentucky Res Found Pferdekrankheitsmodell für herpesviruserkrankungen und verwendungen davon
CN101718740B (zh) * 2009-12-23 2013-12-25 武汉钢铁(集团)公司 一种电子分装仪及其控制方法
CA2871163C (en) 2012-04-23 2020-08-18 Mourik International B.V. Catalyst loading tool
US9604187B2 (en) 2012-04-23 2017-03-28 Mourik International B.V. Particulate material loading device
BR112017023312B1 (pt) 2015-04-29 2022-10-04 Clpros, Llc Aparelho para amortecer e carregar uniformemente um material particulado dentro de um tubo vertical e método para preencher um material particulado em um tubo
CN105126709B (zh) * 2015-09-29 2017-05-10 西南化工研究设计院有限公司 一种用于列管式固定床反应器催化剂的装填装置及装填方法
DK201500657A1 (en) * 2015-10-23 2016-09-05 Haldor Topsoe As Catalyst Loading Method and Apparatus
EP3950114B1 (de) * 2019-03-29 2023-06-07 Mitsubishi Chemical Corporation Verfahren zum laden eines granulierten materials

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GB313168A (de) 1928-06-09 1930-07-24 Skip Compagnie Aktiengesellschaft
US3562998A (en) * 1968-09-17 1971-02-16 Catalyst Services Inc Method for filling vertical process vessels with particulate materials
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US5498731A (en) 1993-06-29 1996-03-12 Mitsubishi Chemical Corporation Oxide catalyst and process for producing maleic anhydride by using oxide catalyst
WO2000044488A1 (fr) 1999-01-28 2000-08-03 Total Raffinage Distribution S.A. Procede et dispositif pour faciliter le remplissage de tubes verticaux a l'aide d'un materiau particulaire
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080298932A1 (en) * 2007-06-01 2008-12-04 Paul Fry Catalyst Loading System
US8025472B2 (en) * 2007-06-01 2011-09-27 Catalyst Services, Inc. Catalyst loading system
US20100175775A1 (en) * 2007-08-13 2010-07-15 Unidense Technology Gmbh Catalyst loading system
US20100218843A1 (en) * 2007-08-13 2010-09-02 Unidense Technology Gmbh process and device for filling a tube with granular material
US8011393B2 (en) * 2007-08-13 2011-09-06 Unidense Technology Gmbh Process and device for filling a tube with granular material
US8550127B2 (en) * 2007-08-13 2013-10-08 Unidense Technology Gmbh Catalyst loading system
US9289740B2 (en) 2007-08-13 2016-03-22 Unidense Technology Gmbh Catalyst loading system
US20090097958A1 (en) * 2007-10-15 2009-04-16 Tubemaster, Inc. Device and method for transporting catalyst to a reactor vessel
US8061524B2 (en) * 2007-10-15 2011-11-22 Extundo Incorporated Device and method for transporting catalyst to a reactor vessel
RU2809250C2 (ru) * 2019-03-29 2023-12-08 Мицубиси Кемикал Корпорейшн Способ загрузки гранул

Also Published As

Publication number Publication date
EP1675675A1 (de) 2006-07-05
TWI336681B (en) 2011-02-01
CN100522334C (zh) 2009-08-05
TW200512146A (en) 2005-04-01
WO2005018791A1 (de) 2005-03-03
US20060233631A1 (en) 2006-10-19
DE10337998A1 (de) 2005-03-17
CA2535357A1 (en) 2005-03-03
ZA200602209B (en) 2007-06-27
CN1835790A (zh) 2006-09-20
AR045276A1 (es) 2005-10-19

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